CN1216058C - Reverse sublimation substance trapping method and its equipment - Google Patents
Reverse sublimation substance trapping method and its equipment Download PDFInfo
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- CN1216058C CN1216058C CN01137835.2A CN01137835A CN1216058C CN 1216058 C CN1216058 C CN 1216058C CN 01137835 A CN01137835 A CN 01137835A CN 1216058 C CN1216058 C CN 1216058C
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- sublimation substance
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- 239000000126 substance Substances 0.000 title claims abstract description 33
- 238000000859 sublimation Methods 0.000 title claims description 31
- 230000008022 sublimation Effects 0.000 title claims description 31
- 238000001926 trapping method Methods 0.000 title description 2
- 238000000034 method Methods 0.000 claims description 39
- 239000000463 material Substances 0.000 claims description 12
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 claims description 6
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 claims description 6
- KMOUUZVZFBCRAM-OLQVQODUSA-N (3as,7ar)-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C=CC[C@@H]2C(=O)OC(=O)[C@@H]21 KMOUUZVZFBCRAM-OLQVQODUSA-N 0.000 claims description 3
- AFPHTEQTJZKQAQ-UHFFFAOYSA-N 3-nitrobenzoic acid Chemical compound OC(=O)C1=CC=CC([N+]([O-])=O)=C1 AFPHTEQTJZKQAQ-UHFFFAOYSA-N 0.000 claims description 3
- QZYCWJVSPFQUQC-UHFFFAOYSA-N 3-phenylfuran-2,5-dione Chemical compound O=C1OC(=O)C(C=2C=CC=CC=2)=C1 QZYCWJVSPFQUQC-UHFFFAOYSA-N 0.000 claims description 3
- GRSMWKLPSNHDHA-UHFFFAOYSA-N Naphthalic anhydride Chemical compound C1=CC(C(=O)OC2=O)=C3C2=CC=CC3=C1 GRSMWKLPSNHDHA-UHFFFAOYSA-N 0.000 claims description 3
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 claims description 3
- 150000004056 anthraquinones Chemical class 0.000 claims description 3
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 3
- 229960003512 nicotinic acid Drugs 0.000 claims description 3
- 235000001968 nicotinic acid Nutrition 0.000 claims description 3
- 239000011664 nicotinic acid Substances 0.000 claims description 3
- PHEDXBVPIONUQT-RGYGYFBISA-N phorbol 13-acetate 12-myristate Chemical group C([C@]1(O)C(=O)C(C)=C[C@H]1[C@@]1(O)[C@H](C)[C@H]2OC(=O)CCCCCCCCCCCCC)C(CO)=C[C@H]1[C@H]1[C@]2(OC(C)=O)C1(C)C PHEDXBVPIONUQT-RGYGYFBISA-N 0.000 claims description 3
- 230000000717 retained effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 88
- 238000001816 cooling Methods 0.000 description 81
- 239000013078 crystal Substances 0.000 description 55
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 description 37
- 239000002826 coolant Substances 0.000 description 24
- 230000002349 favourable effect Effects 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 8
- 238000009826 distribution Methods 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- 238000007599 discharging Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000003507 refrigerant Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 3
- SQNZJJAZBFDUTD-UHFFFAOYSA-N durene Chemical compound CC1=CC(C)=C(C)C=C1C SQNZJJAZBFDUTD-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005194 fractionation Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 206010020843 Hyperthermia Diseases 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 235000019628 coolness Nutrition 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 235000012489 doughnuts Nutrition 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000036031 hyperthermia Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Images
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
- F28D7/00—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
- F28D7/16—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being arranged in parallel spaced relation
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
- F28D7/00—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
- F28D7/0066—Multi-circuit heat-exchangers, e.g. integrating different heat exchange sections in the same unit or heat-exchangers for more than two fluids
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
- F28D7/00—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
- F28D7/0066—Multi-circuit heat-exchangers, e.g. integrating different heat exchange sections in the same unit or heat-exchangers for more than two fluids
- F28D7/0083—Multi-circuit heat-exchangers, e.g. integrating different heat exchange sections in the same unit or heat-exchangers for more than two fluids with units having particular arrangement relative to a supplementary heat exchange medium, e.g. with interleaved units or with adjacent units arranged in common flow of supplementary heat exchange medium
- F28D7/0091—Multi-circuit heat-exchangers, e.g. integrating different heat exchange sections in the same unit or heat-exchangers for more than two fluids with units having particular arrangement relative to a supplementary heat exchange medium, e.g. with interleaved units or with adjacent units arranged in common flow of supplementary heat exchange medium the supplementary medium flowing in series through the units
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S55/00—Gas separation
- Y10S55/15—Cold traps
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
A reversely subliming substance is efficiently collected on a commercial scale from a gas containing the substance. This is achieved by introducing the gas containing the substance into a shell-and-tube collecting apparatus by controlling the resistance offered to the gas during the passage thereof through the cooled tubes retained inside the collecting apparatus or by utilizing gas-introducing tubes excelling in dispersibility.
Description
Technical field
The present invention relates to a kind of equipment that from the gas that contains reverse sublimation substance, captures the method for reverse sublimation substance and be used for this capture.
Background technology
For being that raw material carries out the method that catalytic vapor phase oxidation reaction synthesizes PMA and capture PMA from contained output gas with for example durol, delivered various report so far.Available have several as shown below methods of utilizing cooling stave surface to obtain the brilliant PMA of big burl.
U.S.4,252,545 have disclosed a kind of method, comprise make contain PMA gas with 1-3 meter per second flow velocity parallel-flow through remaining on the cooling surface of equilibrium temperature, and reclaim formed thus crystal grain with the technology of fractionation up reversal China.This method comprises two kinds of schemes, and a kind of gas that makes flow to downwards in many pipes, and another kind of scheme makes the heat exchange surface of gas stream to board-like solidification device.Basically, this method is as much as possible to avoid to degree crystal grain to be deposited on the cooling stave surface.Sedimentary thus crystal grain is regularly stripped down with washing or mechanical means again thereon fast.This method causes the relevant devices operational difficulty.
U.S.3,693,707 have disclosed and a kind ofly utilize finned tube to make to contain the gas up reversal China of PMA to separate out crystalline equipment.This equipment proves a kind of commercial very expensive equipment undoubtedly, because these crystal grain are in case attached on the complex surface, such as on the surface of this finned tube, be difficult for peeling off and reclaiming.
JP-B-61-121 has disclosed a kind of method and its equipment, comprise making and contain PMA gas up reversal China, impel this sour crystal grain on the cooling stave surface, to deposit and grow up, the temperature of wall surface raise then to surpassing its sublimation temperature, thereby remove the crystal grain that adheres to by distillation, and impel the residual crystal grain of growing up to leave wall surface and fall.But this method has caused that equipment is complicated and make the problem that loss strengthens that captures because of the crystal grain that distils.
JP-A-4-131,101 have disclosed a kind of method, comprise making the airflow that contains the compound that distils carry attrition resistant particle secretly, thereby are luring into the sedimentary while on the cooling surface of crystal grain at condenser, make abrasion resistant particles collision crystal grain, make it be broken into powdery.But, this method caused product only for powdery and equipment because of the frayed problem of particles hit.
JP-A-10-265,474 have disclosed a kind of method, comprise impelling crystal grain to precipitate on the cooling surface of upright tubular(surface)condenser, and the surface temperature that raises then makes crystal grain owing to sublimation pressure is stripped from.JP-A-10-279,522 have disclosed a kind of method, comprise and impel crystal grain to precipitate on cooling surface, reduce surface temperature then, make crystal grain owing to surface and intercrystalline difference in shrinkage are peeled off.In this description of the invention, do not mention any realistic model, about the shell-tube type trap of industrial effective this method of running.
Therefore, known also without any method, be enough to direct reverse sublimation substance, such as producing PMA from gas phase industrial production high purity and volume particle size.
Summary of the invention
The object of the invention is to provide a kind of method and equipment thereof that reclaims reverse sublimation substance, method is by fractionation up reversal China, from the gas that contains reverse sublimation substance, reclaim this material,, wherein discharge high purity and the abundant crystal grain that captures from trapping system such as PMA.
A kind of method that reaches the object of the invention is, utilize a kind of its cold-trap pipe internal surface can adhere and capture the shell-tube type trap of reverse sublimation substance, from the gas that contains this material, capture reverse sublimation substance, wherein adjustments of gas pass cooling tube the pressure-losses at 0.05-50, the scope of 000Pa (handkerchief).
Also can reach a kind of method of the object of the invention is, utilize a kind of its cold-trap pipe internal surface can adhere and capture the shell-tube type trap of reverse sublimation substance, capture contains the reverse sublimation substance in this material gas, wherein has one to be used for the public space that is made of the trap bottom of gas inlet tube and to make gas introduce this space with one of following at least means in the cooling tube:
(1) gas inlet tube, there is a porous plate at its outlet position,
(2) gas inlet tube, the direction that its Way out passes cooling tube with respect to gas have one greater than 90 ° angle, and
(3) two or more root gas inlet tubes.
In addition, reach the also adoptable method of the object of the invention and be, be used for adhering and capturing this material that contains reverse sublimation substance gas by means of a shell-tube type equipment, wherein the cooling tube exit portion that constitutes in the shell-tube type equipment all is equipped with baffle plate separately.
According to method of the present invention, might make the gas flow equalization that contains reverse sublimation substance of passing each cooling tube, and can pass under the pressure-losses that is fixed in the cooling tube in the shell-tube type trap at the gas of regulation, regulate resistance to improve collecting coefficient to this material.
According to method of the present invention, can make and pass the gas flow equalization that contains reverse sublimation substance that is fixed in each cooling tube in the shell-tube type trap, and can make the collecting coefficient of this material is improved, because utilizing the shell-tube type trap gas is effectively disperseed in to its capture process.
According to trap of the present invention, might make the gas flow equalization that contains reverse sublimation substance of passing each cooling tube, and gas is introduced in the trap of the gas inlet tube that has strong dispersed gas physical efficiency power, and on each spout member of the cooling tube in being fixed in trap baffle plate is set, thereby controlled chilling pipe resistance is to improve the collecting coefficient to this material.
According to following description to preferred embodiment, above other purpose, characteristics and the advantage of reaching of the present invention all can seem more clear.
Brief Description Of Drawings
Add and constitute this specification sheets part description of drawings several aspects of the present invention, together with the description, principle of the present invention has been described also.In the figure:
This figure is explanation captures an example of reverse sublimation substance equipment according to the present invention a sectional view.
Embodiment
Referring now to accompanying drawing to the method that captures reverse sublimation substance or desublimation material according to the present invention with carry out the equipment describe that captures in down.Accompanying drawing is the sectional schematic diagram that width of cloth explanation the present invention is used to capture the equipment of reverse sublimation substance.Each pipe that appears among the figure is overweening in order to set forth this specification sheets.Here used term " reverse sublimation substance " refers to and a kind ofly can be converted into solid-state sublimate from steam-like.The example of this sublimate can comprise PMA, Tetra hydro Phthalic anhydride, maleic anhydride, anthraquinone, naphthalic anhydride, M-nitro benzoic acid, phenyl maleic anhydride, phenanthrene and nicotinic acid.Among the above-mentioned sublimate, it is especially suitable that PMA proves.The present invention will quote PMA as its type case description in down.
Be not particularly limited containing PMA gas, and only require and contain PMA.Usually, this gas preferably contains by with the durol being the PMA (can be described as " PMDA ") that raw material carries out catalytic vapor phase oxidation reaction and obtains.Various known catalyzer all can be used for this reaction.Contain vanadium and the silver catalyzer as principal constituent, its silver is 0.0001-0.2 to the vanadium atom ratio: 1, can quote as an example.
The above-mentioned general concentration of gas of reverse sublimation substance that contains is at 5-50g/Nm
3Scope is preferably at 15-35g/Nm
3The reverse sublimation substance of scope.
The gas that contains PMDA is incorporated into the lower space 5 of upright shell-tube type catching apparatus or trap 1 via gas inlet tube 3.Here used term " upright shell-tube type trap " refers to and is provided with two or the pipe of more fixed diameters or a kind of equipment of trap tube in the cooling tower, and this equipment keeps the wall surface of these pipes to be subjected to the cooling of cooling agent, thereby, make material cooling by this cold-trap pipe by means of the heat exchange between this material and cooling tube inner wall surface.The cooling tube that word " uprightly " means this equipment is parallel to gravity direction, wherein the crystal grain of deviating to peel off from cooling tube by gravity.The space 5 that is used for gas inlet tube 3 is positioned at the bottom of trap 1, and is surrounded with the bottom of many cooling tubes 10,11 and 12, the lower wall and the crystal grain dumping device 19 of trap 1 all around.In this structure, preferably, be that gas inlet tube is provided with porous plate and settles gas inlet tube in its exit portion, make the discharging direction with respect to the dispersion angle of the gas direction formation of passing cooling tube, and many gas inlet tubes are set greater than 90 °.Adopt this method can guarantee to contain PMDA gas and directly do not enter cooling tube, and can make the gas dispersion and the uniform distribution that contain PMDA pass through cooling tube.
The general porous plate of installing makes the pressure-losses be lower than 10,000Pa, and preferably at 100-5, the scope of 000Pa is although the eyelet number depends on the amount of flowing gas and the size of trap.To the shape of the eyelet that forms on the porous plate without limits, can be chosen as circle, trilateral, tetragon and rectangle arbitrarily.
The angle of settling gas inlet tube to make its gas discharge direction to constitute with respect to the gas direction of passing cooling tube 10,11 and 12 is greater than 90 °, preferably 90 °-270 ° scope, more preferably 120 °-240 ° scope.It is fine to utilize this gas inlet tube that the gas dispersion that contains reverse sublimation substance is got.Have two kinds of methods can change the discharge direction: a kind of method is with the direct fixed gases inlet tube of predetermined angular, or another kind of method is to connect other pipe in the gas inlet tube outlet.For the little trap of diameter, the latter is more effective, because can be little for the space.
In addition, from improving, this trap is advantageously installed many gas inlet tube 3a and 3b, the i.e. scope of 2-10 root to introducing the viewpoint of gas dispersion ability.For the occasion that many gas inlet tube 3a and 3b have been installed, allow that they are taken over the meaning position and settle and form any dispersion angle, and every pipe forms the airshed of different volumes.From control dispersive ability viewpoint, make gas inlet tube 3a and 3b to equate that the even arrangement of dispersion angle in one plane is favourable.For occasion with two gas inlet tube 3a and 3b, make they with etc. dispersion angle in one plane be favourable each other substantially on the contrary.
Then, make and contain PMDA gas by gas inlet tube 3a, b, enter in the trap 1 that many cooling tubes 10,11 and 12 are housed in it, make and disperse gas to enter in cooling tube 10,11 and 12, wherein PMDA is separated from the gas and be deposited on the internal surface of cooling tube 10,11 and 12.Suitably, cooling tube diameter (internal diameter) is bigger, generally in 100-500 millimeter scope, preferably in 150-400 millimeter scope, more preferably in 150-300 millimeter scope.If 100 millimeters of cooling tube internal diameter less thaies then cause separation and reclaim the crystal grain difficulty that is captured.Otherwise,, then have the shortcoming that reduces the PMDA collecting coefficient if internal diameter surpasses 500 millimeters.The used pipe range of the present invention is not particularly limited, but can be 3,000-6,000 millimeter scope.If length is too short, then can not fully reclaim desired substance.Otherwise, if length is oversize, then can increase facility investment, and its productive rate can be not high yet.Yet the pipe caliber of conventional shell and tube heat exchanger is less, and for example 25.4 millimeters, purpose is in order to improve the heat-exchange capacity of unit volume interchanger.
In addition, for the occasion of the temperature distribution that will slow down cooling agent, it is favourable that baffle plate (for example otch is 25%) or a kind of disc and doughnut baffle are set in refrigerant circuits.When (not indicating) order that made progress by downside is settled annular, disc and ring baffle, cooling agent rises on the hole by ring baffle, follow horizontal flow between annular and disk baffle, rise along the trap sidewall between disk baffle peripheral part and trap, horizontal flow between disk and ring baffle then, rising in hole by ring baffle, and keeps same mobile after this again.Flow along the sidewall direction in the above-mentioned trap because this cooling agent is inevitable, this just can suppress especially along horizontal temperature distribution.Owing to suppressed temperature distribution as mentioned above, just might make the more all even quality of sedimentary crystal grain on the cooling tube internal surface that makes of these pipe coolings disperse (qualitydispersion) to reduce.
In trap, use these baffle plate parts, because the cooling agent along continuous straight runs flows, so the outlet and the inlet that multiple spot cooling agent are set along the trap peripheral part are favourable, so that further slow down the temperature distribution of cooling agent.With comparing that introduce a position, multiple spot is introduced the refrigerant temperature distribution is more slowed down, because cooling agent is to introduce by the whole periphery of trap basically.Equally, when discharging cooling agent, as mentioned above, use the temperature distribution that to slow down cooling agent with quadrat method by trap.Owing to suppressed the temperature distribution of cooling agent in the trap as mentioned above, the quality of sedimentary crystal grain disperses to be slowed down on the cooling tube internal surface.
Gas outlet in cooling tube 10,11 and 12 is preferably respectively installed baffle plate 14,15 and 16, so that regulate cooling tube 10,11 and 12 resistances that constituted.Baffle shapes is not particularly limited, but can be included in its top that the centre forms the baffle plate in specified diameter hole and be placed in cooling tube upper end respectively by the cone that cuts.Suitably, the pressure-losses is generally at 0.05-50, the 000Pa scope, and preferably at 1-10, the 000Pa scope.If the not enough 0.05Pa of the pressure-losses, then shortcoming is fully not keep air-flow homogeneous in each cooling tube.Otherwise, if the pressure-losses surpasses 50,000Pa, then excessive shortcoming is to require the gas blower ability too high, thereby requires additional investment, does not but obtain any particular advantage.
Make the gas dispersion that contains reverse sublimation substance in the trap lower space, and do not make the discharge direction of gas inlet tube directly face toward cooling tube, and also control the resistance of each cooling tube, just might make the linear speed equalization of air-flow in each cooling tube.V-bar is generally in the 0.05-1Nm/sec scope in the cooling tube, preferably in the 0.05-0.5Nm/sec scope. follow this scope, just can reach the effect of avoiding to depart from 0.065Nm/sec, it is 50% value of average linear speed 0.13Nm/sec in the cooling tube, with depart from 0.195Nm/sec, 150% value of promptly average linear speed.
In trap 1, the temperature of the wall surface that is in space 17 is remained on be higher than the precipitated temperature of PMDA crystal grain.Adopt comparatively high temps, might prevent the crystal grain precipitation and prevent that the crystal grain that baffle plate 14,15 and 16 perforations are fallen stops up, thereby can make the long-term continuous service of operation.
The part PMDA crystal grain that is attached to cooling tube 10,11 and 12 is emanated naturally and is fallen.Vibration or bump device 21a and 21b are installed to promoting that this separation is effective on each site of trap 1 outer periphery arrangement cooling tube.Although the bump device can be interrupted or centralized operation, from the energy efficiency viewpoint, because crystal grain lands naturally, after crystal grain was focused to certain degree, it was favourable carrying out centralized operation.The several bump devices of general installation are favourable, but the bump device count of adorning becomes with trap size and collision efficiency.Position to the bump device is not particularly limited, but considers to strengthen the die separation effect, and it is placed on the tube sheet.In addition, refrigerant temperature rise to be higher than cooling temperature such as 250 ℃ after, or be reduced to lowlyer as after 30 ℃ than process of cooling temperature, begin operation bump device, may promote the separation of deposition crystal grain on the cooling tube.Although the isolating mechanism of this promotion is not also proved absolutely, but can infer and be interpreted as, the temperature difference on the cooling tube between sedimentary grain surface layer and pipe thermal expansion place has produced the tension force effect to great number of grains, makes the fracture of precipitation crystal grain layer, thereby has promoted the crystal grain landing.
The crystal grain of having emanated and having landed accumulates in the bottom or the bottom of trap.Accumulative crystal grain is acicular by this way, so flowability is not good, so that it discharges difficulty.We have further studied a kind of method that can make in the crystal grain discharge trap of emanating.Therefore, have found that, the trap bottom is constituted with the horizontal direction angle be not less than 30 ° taper shape, for example preferred 50-80 °, can make that crystal grain lands fast in the trap, and make further that trap 1 equipment is a kind of might to help trap to emit crystal grain to assembling discharging device 19 that crystal grain directly applies reactive force as the circle feeding machine.When discharging device 19 itself does not possess the function of blocking with the trap environment, the discharging that has securing device device need be provided separately, spill and prevent air and foreign matter intrusion trap to prevent gas from trap.
Cooling tube that is placed in the trap bottom and conical side wall to direct contact PMDA crystal grain carry out milled processed, the relative roughness that makes it to reach by Ry (JIS (Japanese Industrial Standards) B0601 1994) standard setting is 9.8 μ m, preferred 5 μ m, more preferably 1 μ m is to satisfy the function that promotes to separate and reclaim crystal grain.Polishing method is not particularly limited in operation.Can quote polishing technology and electropolishing technology as an example.
The gas that passes cooling tube partly contains PMDA.It is concentrated in trap 1 upper space 17, handled by waste gas burner (not indicating) then, burning is wherein such as the combustiblesubstance of PMDA.Optional, before waste-gas burning, can carry out the secondary capture to this gas for capturing PMDA.Secondary captures available capture instrument such as cyclonic separator, bag type filter, washing column or moistening tower and finishes.
According to the present invention, can obtain crystal grain than volume particle size.
Embodiment
Refer now to embodiment the present invention is illustrated, but non-these embodiment that is limited to of the present invention.
Embodiment 1
Trap shown in the figure is suitable at following conditional operation.
(catching apparatus general introduction)
(i) polishing (cooling tube internal surface): electropolishing
4,000 millimeters of 200 millimeters of internal diameters and length
An orifice plate respectively is equipped with on the pipe top, its thick 2 millimeters and comprise the eyelet of 80 millimeters of diameters.
(ii) PMDA gas inlet tube: the gas inlet tube exit end of under the shell-tube type trap, settling in the space, two bend pipes that are 180 ° of angles with respect to the direction of passing cooling tube gas of fit on.
The (iii) cooling tube length of extending: 100 millimeters from lower tubesheet
(iv) solvent 1: from the cooling tube length of cooling tube gas inlet cooling 15%.
(v) solvent 2: cooling cooling tube rest part.
(the vi) angle of trap lower cone body portion: be 50 ° of angles with level.
(the vii) Ry:1 μ m of trap lower cone part.
Finish capture according to following method.That to form by the durol gaseous oxidation and to contain PMDA concentration be 33.2g/Nm
3Gas send in the trap via the PMDA gas inlet tube, its volumetric flow rate should make that gas line speed is 0.3Nm/sec in the trap.At this moment, the pressure-losses that gas passes in the cooling tube process is 0.1Pa, and the gas inlet and the pressure-losses that is arranged between the orifice plate at cooling tube top are 2,000Pa.Trap introduced contained PMDA gas 24 hours, the temperature that keeps cooling agent 1 in the temperature of 195 ℃ and cooling agent 2 at 170 ℃.After this, start the bump device, desorption is attached to the PMDA on the cooling tube, and makes it to drop out.The PMDA amount that is drawn off by the discharging parts that are placed in the trap bottom is 72 weight % (recovery percent), and the purity that reclaims crystal grain is 99.9%.
Press the identical condition of aforesaid operations, continued the operation trap again 5 days.Behind 5 days EOs, stop trap being carried containing PMDA gas, and the temperature that changes cooling agent 1 and 2 is all to 30 ℃.After this start the bump device, the crystal grain that is attached on the pipe falls, and its purity is 99.9%.
The average recovery percent of 6 days period P MDA comprises fallen crystal grain, is 85.5 weight %.PMDA crystal grain is needle-like, and mean particle size is 400 μ m.
V-bar reaches the ratio injection air of 0.13Nm/sec in the cooling tube in making, and measures the exit linear velocity of each cooling tube.Each pipeline speed do not reach i.e. 50% average linear velocity of 0.065Nm/sec, or surpasses i.e. 150% average linear velocity of 0.195Nm/sec.Maximum is 121% average linear velocity, and Schwellenwert is 64.7% average linear velocity.
Comparative Examples 1
(saving orifice plate)
Repeat the step of embodiment 1, but different be the whole orifice plates that saved the cooling tube top.Equally trap is introduced and contained PMDA gas 24 hours.The PMDA recovery percent that removes with the bump device is 66 weight %.
Continued the operation trap under the same conditions again 5 days, and stopped then trap sent into and contain PMDA gas, and change cooling agent 1 and 2 the two temperature all to 30 ℃.Start the bump device, the result falls other crystal grain.Crystal grain purity 99.9%.
The average recovery percent of PMDA comprises that fallen crystal grain is 75 weight % in 6 day phase.PNDA crystal grain is aciculiform.
After taking off orifice plate from trap, provide air in the ratio that can make V-bar in the cooling tube reach 0.13Nm/sec to it, and measure the gas line speed at each cooling tube top.Each cooling tube interior lines underspeed 0.065Nm/sec's, promptly 50% average linear velocity accounts for 22% of all speed, and surpass 0.195Nm/sec, and promptly 150% average linear velocity accounts for 30% of all speed.Maximum is 243% average linear velocity, and Schwellenwert is 24.3% average linear velocity.
Comparative Examples 2
(saving orifice plate and gas inlet tube)
Repeat the step of embodiment 1, but different be to have saved whole orifice plates at cooling tube top and saved the PMDA gas inlet tube.Equally trap is introduced and contained PMDA gas 24 hours.The PMDA recovery percent of deviating from the bump device is 55 weight %.
Continued the operation trap under the same conditions again 5 days, and stopped then trap introduced and contain PMDA gas, change cooling agent 1 and 2 the two temperature then all to 30 ℃.Start the bump device, the result falls other crystal grain.The purity of crystal grain is 99.9%.
The average recovery percent of PMDA comprises that fallen crystal grain is 65 weight % in 6 day phase.PMDA crystal grain is aciculiform.
Take out in the trap behind the orifice plate and elbow part, set the ratio that V-bar reaches 0.13Nm/sec in the cooling tube and provide air in making, and measure the linear speed of each cooling tube exit portion to it.Gas line speed not enough 0.065Nm/sec in each cooling tube, promptly 50% average linear velocity accounts for 53% of whole speed, and surpass 0.195Nm/sec, and promptly 150% average linear velocity accounts for whole speed 31%.Maximum is 284% average linear velocity, and Schwellenwert is 20.1% average linear velocity.
Claims (4)
1, a kind of method that from the gas that contains reverse sublimation substance, captures reverse sublimation substance, method is to utilize the shell-tube type catching apparatus (1) that can adhere and capture this material on a kind of internal surface of cold-trap pipe, wherein said reverse sublimation substance is selected from PMA, Tetra hydro Phthalic anhydride, maleic anhydride, anthraquinone, naphthalic anhydride, M-nitro benzoic acid, the phenyl maleic anhydride, phenanthrene and nicotinic acid, this method is characterised in that, adjusting is passed the pressure-losses of the gas that contains this material of trap tube at 0.05-50, the scope of 000Pa and/or this trap tube have one and are used for the public space (5) that constitutes in the catching apparatus bottom of gas inlet tube (3) and make gas introduce this space with one of following at least method:
(1) gas inlet tube (3) has porous plate at its export department's bit strip,
(2) gas inlet tube (3), its Way out pass the angle of direction of trap tube greater than 90 ° with respect to gas, and
(3) two or more gas inlet tubes (3).
2, according to the process of claim 1 wherein that this trap tube is equipped with the baffle plate that can cause the pressure-losses separately in its exit portion.
3, a kind of shell-tube type catching apparatus (1) that can from the gas that contains reverse sublimation substance, adhere and capture reverse sublimation substance, wherein said reverse sublimation substance is selected from PMA, Tetra hydro Phthalic anhydride, maleic anhydride, anthraquinone, naphthalic anhydride, M-nitro benzoic acid, phenyl maleic anhydride, phenanthrene and nicotinic acid, this apparatus characteristic is to have the trap tube spout member in the equipment that is arranged at the band baffle plate.
4, according to the equipment of claim 3, wherein trap tube has the public space that is used for gas inlet tube (3) (5) that constitutes in the bottom of catching apparatus (1), and the Way out of gas inlet tube (3) passes the angle of direction of trap tube greater than 90 ° with respect to gas.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP340759/2000 | 2000-11-08 | ||
| JP340759/00 | 2000-11-08 | ||
| JP2000340759A JP3949371B2 (en) | 2000-11-08 | 2000-11-08 | How to collect reverse sublimable substances |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1353110A CN1353110A (en) | 2002-06-12 |
| CN1216058C true CN1216058C (en) | 2005-08-24 |
Family
ID=18815621
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN01137835.2A Expired - Fee Related CN1216058C (en) | 2000-11-08 | 2001-11-08 | Reverse sublimation substance trapping method and its equipment |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US6638345B2 (en) |
| EP (1) | EP1205479A1 (en) |
| JP (1) | JP3949371B2 (en) |
| CN (1) | CN1216058C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106178577B (en) * | 2015-05-05 | 2017-12-15 | 江苏宇通干燥工程有限公司 | Sublimate device and its method of work |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004067527A (en) * | 2002-08-02 | 2004-03-04 | Nippon Shokubai Co Ltd | Method for recovering sublimable substance |
| JP2005035959A (en) * | 2003-07-18 | 2005-02-10 | Nippon Shokubai Co Ltd | Method for producing maleic anhydride |
| DE102005031660A1 (en) * | 2005-07-05 | 2007-01-11 | Coperion Waeschle Gmbh & Co. Kg | Apparatus for heating or cooling bulk material comprises a tube and shell heat exchanger and a system for reheating or recooling a heat transfer liquid supplied to the shell side |
| CN107401938B (en) * | 2016-05-18 | 2019-08-23 | 王彩虹 | A kind of gas-particle two-phase heat exchange equipment |
| EP3715762A1 (en) * | 2019-03-28 | 2020-09-30 | Valeo Autosystemy SP. Z.O.O. | A heat exchanger |
| CN112944936A (en) * | 2019-12-14 | 2021-06-11 | 黄相兰 | Condensing system and method for new material processing production |
| CN115738348B (en) * | 2022-11-14 | 2024-08-13 | 中国科学院过程工程研究所 | Anti-blocking cooling crystallizer, cooling crystallization method and application thereof |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2189173A (en) * | 1938-07-09 | 1940-02-06 | Dow Chemical Co | Recovery of gaseous diolefins |
| US2602647A (en) * | 1951-03-30 | 1952-07-08 | Standard Oil Co | Tubular contactor with conical distribution plate |
| CH472364A (en) | 1966-12-22 | 1969-05-15 | Geigy Ag J R | Process for the preparation of a new polycyclic amine |
| JPS52142675A (en) | 1976-05-22 | 1977-11-28 | Kazuo Minai | Method and apparatus for getting crystal of sublimate |
| DE2751979A1 (en) | 1977-11-22 | 1979-05-23 | Huels Chemische Werke Ag | PROCEDURE FOR FRACTIONAL DESUBLIMATION OF PYROMELLITIC ACIDIAN HYDRIDE |
| JPS6438590A (en) * | 1987-08-04 | 1989-02-08 | Toshiba Corp | Heat exchanger |
| JPH04131101A (en) | 1990-09-20 | 1992-05-01 | Nippon Steel Chem Co Ltd | Sublimable compound collecting method |
| JP3967417B2 (en) | 1997-03-21 | 2007-08-29 | 株式会社日本触媒 | Method for recovering pyromellitic anhydride |
| JP3908325B2 (en) | 1997-04-07 | 2007-04-25 | 株式会社日本触媒 | Recovery method for sublimable substances |
-
2000
- 2000-11-08 JP JP2000340759A patent/JP3949371B2/en not_active Expired - Fee Related
-
2001
- 2001-11-01 US US10/008,258 patent/US6638345B2/en not_active Expired - Fee Related
- 2001-11-07 EP EP01204277A patent/EP1205479A1/en not_active Withdrawn
- 2001-11-08 CN CN01137835.2A patent/CN1216058C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106178577B (en) * | 2015-05-05 | 2017-12-15 | 江苏宇通干燥工程有限公司 | Sublimate device and its method of work |
Also Published As
| Publication number | Publication date |
|---|---|
| US20020053288A1 (en) | 2002-05-09 |
| US6638345B2 (en) | 2003-10-28 |
| CN1353110A (en) | 2002-06-12 |
| JP3949371B2 (en) | 2007-07-25 |
| JP2002143604A (en) | 2002-05-21 |
| EP1205479A1 (en) | 2002-05-15 |
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